CN108570850B - Preparation method of super-wetting woven fabric with excellent stability and tolerance for oil-water separation - Google Patents

Preparation method of super-wetting woven fabric with excellent stability and tolerance for oil-water separation Download PDF

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CN108570850B
CN108570850B CN201810152526.XA CN201810152526A CN108570850B CN 108570850 B CN108570850 B CN 108570850B CN 201810152526 A CN201810152526 A CN 201810152526A CN 108570850 B CN108570850 B CN 108570850B
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CN108570850A (en
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郭志光
高晓宇
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Hubei University
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    • D—TEXTILES; PAPER
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
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    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
    • D06M13/21—Halogenated carboxylic acids; Anhydrides, halides or salts thereof
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    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/11—Oleophobic properties
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    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
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    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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Abstract

The invention relates to a preparation method of a super-wetting woven fabric with excellent stability and tolerance for oil-water separation. The research realizes super-hydrophobic, super-hydrophilic and super-amphiphobic performances by controlling the growth of zinc oxide on the woven fabric and selecting different modifiers, and has good stability under heating, acid-base, abrasion experiments and ultraviolet irradiation. In addition, the paper can be used for separating oil-water mixture, not only can realize the separation of light oil, heavy oil and water, but also can realize the separation of oil and water according to the requirement. The preparation method disclosed by the invention is simple in preparation process, controllable, easy to obtain, strong in stability, suitable for large-area preparation and application, suitable for application in daily life, and also suitable for industrial fields such as oil-water separation and the like.

Description

Preparation method of super-wetting woven fabric with excellent stability and tolerance for oil-water separation
Technical Field
The invention belongs to the technical field of preparation of super-hydrophobic woven fabrics, super-hydrophilic woven fabrics and super-amphiphobic woven fabrics, and particularly relates to a preparation method for preparing stable super-wetting woven fabrics with excellent tolerance and capable of being used for oil-water separation.
Background
The phenomenon of super-wetting, especially super-hydrophobic phenomenon, is widespread in nature, such as lotus leaf surface, butterfly wing, water strider leg, etc. The contact angle of the surface of the super-hydrophobic material to water is more than 150 degrees, and the rolling angle is less than 10 degrees. Superhydrophobic materials have many unique and excellent surface properties: the characteristics of hydrophobicity, self-cleaning property, corrosion resistance, anti-icing property, anti-fog property and the like enable the paint to have huge application prospect in a plurality of fields.
The realization of oil-water separation is one of the great applications of super-hydrophobicity. The realization of oil-water separation has important significance for reducing the influence of moisture and impurities on the quality of oil, solving the problem of pollution of water-insoluble oil stains to rivers, lakes and seas and the like. By utilizing the special wettability of super-hydrophobicity, oil can smoothly pass through but water can not pass through, and the oil-water mixture can be effectively separated. There are now a number of researchers applying superhydrophobicity to oil-water separation. Chinese patent CN101708384A adopts wet chemical etching technology to prepare nano-scale microscopic protrusions on the surface of a metal mesh with micron-sized apertures, and then modifies a compound with low surface energy on the surface of the metal mesh, thereby preparing the metal mesh with super-hydrophobic property, and effectively realizing oil-water separation. Chinese patent CN101518695A adopts a dip-coating method, uses certain conditions and curing agents to copolymerize epoxy-terminated oligosiloxane and bisphenol A, uniformly mixes the polysiloxane-bisphenol A copolymer and the curing agents to prepare a solution, and cures the polysiloxane-bisphenol A copolymer on a 100-400 mesh fabric net to prepare the oil-water separation net film with super-hydrophobic and super-oleophylic functions. Although the technical scheme has the oil-water separation effect, the method has the defects that the preparation method is complex, the prepared super-hydrophobic base material has poor stability and cannot be repeatedly used, or a metal net is used as the base material, so that the cost is high, the universality is not realized, and the like.
Disclosure of Invention
The invention aims to provide a simple and convenient method for industrially producing super-hydrophobic, super-hydrophilic and super-amphiphobic woven fabrics, and solves the problems of complicated preparation steps, poor weather resistance, low practicability and poor wear resistance of a super-wetting material. The super-hydrophobic and super-hydrophilic woven fabric with good stability, wear resistance, ultraviolet resistance, acid and alkali resistance and high temperature resistance is prepared by a simple method, and the obtained super-hydrophobic and super-hydrophilic woven fabric has good oil-water separation capability.
The invention adopts a pretreatment-growth hydrothermal two-step method to enable the ZnO nano-array to grow on the surface of the fiber woven fabric, and the length-diameter ratio of the ZnO nano-rod array is controlled by changing the concentration of a crystal growth solution, thereby preparing the ZnO nano-rod and the nano-needle. In order to improve the adhesion of the crystal layer to the surface of the fabric substrate, two silane coupling agents (hydrophobic TTOP-12 and hydrophilic KH550) are selected and added into the pretreatment solution to prepare a surface with special wettability. According to different choices of changing the type of the silane coupling agent, controlling the ZnO crystal form and the low surface energy modifier, the super-hydrophobicity, super-hydrophilicity, super-amphiphobicity and other wettabilities of the fiber fabric are successfully realized. For practical production applications, the resistance and durability of such surfaces under different test environments, including mechanical properties, chemical properties, high temperature properties and ultraviolet irradiation, were studied and measured. The oil-water separator can efficiently separate oil and water according to needs by utilizing the difference of water and oil wettability, has great flexibility, and is expected to be used for treating oil-water mixtures.
The technical scheme for realizing the purpose of the invention is as follows: a method for producing a super-wet woven fabric having excellent stability and resistance for oil-water separation, comprising the steps of:
A. pretreatment of weaving: weighing zinc acetate, adding the zinc acetate into isopropanol, heating and stirring, dissolving, adding triethylamine, mixing to form a milky white solution, and cooling to room temperature; then weighing the solution, adding a hydrophobic silane coupling agent TTOP-12, stirring and mixing to form a mixed solution A, or adding a hydrophilic silane coupling agent KH550, stirring and mixing to form a mixed solution B, adding the solution A or the solution B into the ultrasonically cleaned woven fabric, soaking for 5min, taking out, and airing at 120 ℃ for later use;
B. and (3) growth of nano zinc oxide: preparing zinc nitrate and hexamethylenetetramine aqueous solution with equal concentration, mixing the solution with equal volume, stirring the solution for 30min to obtain a zinc oxide growth solution, vertically putting the pretreated woven fabric into the growth solution, reacting the solution in an oil bath at 95 ℃ for 8h, and standing the solution at normal temperature for 12h to finish the growth of the nano zinc oxide;
C. low surface energy substance modification: taking out the woven fabric in the step B, repeatedly washing with distilled water and then drying;
if the hydrophilic silane coupling agent KH550 is added in the pretreatment, the super-hydrophilic woven fabric can be obtained without further treatment;
if the hydrophobic silane coupling agent TTOP-12 is added in the pretreatment, then the woven fabric is immersed in the stearic acid ethanol solution for 2 hours to obtain the super-hydrophobic performance; or if the hydrophilic silane coupling agent KH550 is added in the pretreatment, soaking the woven fabric into the perfluorooctanoic acid ethanol solution for 24 hours to obtain the super-amphiphobic property; and then taking out the woven fabric, washing the woven fabric with absolute ethyl alcohol, and drying the woven fabric in a vacuum drying oven at 60 ℃ to obtain the super-hydrophobic woven fabric or the super-amphiphobic woven fabric.
Furthermore, the concentrations of zinc acetate and triethylamine in the pretreatment solution were both 0.1 mol/L.
Further, the ratios of the silane coupling agent TTOP-12 and the silane coupling agent KH550 to the pretreatment solution added were 1.5 w% and 2 w%, respectively.
Further, in the growth solution of the super-hydrophobic woven fabric, the optimal concentration of the zinc nitrate aqueous solution and the hexamethylene tetramine is 0.15 mol/L.
Further, in the growth solution of the super-hydrophilic woven fabric, the optimal concentration of the zinc nitrate aqueous solution and the hexamethylenetetramine is 0.05 mol/L.
Further, in the growing solution of the super-amphiphobic woven fabric, the optimal concentration of the zinc nitrate aqueous solution and the hexamethylene tetramine is 0.025 mol/L.
Further, the concentration of the ethanol solution of stearic acid was 0.05 mol/L.
Further, the concentration of the ethanol solution of perfluorooctanoic acid was 0.005 mol/L.
The invention has the beneficial effects that: compared with the prior art, the invention has the advantages that:
1. the process is simple, the raw materials are easy to obtain, and the cost is low;
2. the prepared super-hydrophobic and super-hydrophilic fabric has good wear resistance, chemical stability, heat resistance and ultraviolet resistance;
3. the prepared super-hydrophobic fabric has super-hydrophobic/super-oleophilic properties, the contact angle of water is more than 150 degrees, the rolling angle is less than 10 degrees, the contact angle of oil is about 0 degree, the super-hydrophilic fabric has underwater super-oleophobic/oil-down super-hydrophobic properties, the contact angle of oil in water is more than 150 degrees, and the contact angle of water in oil is more than 150 degrees;
4. the super-hydrophobic and super-hydrophilic woven fabric can be used for oil-water separation;
5. the super-wetting fabric has high mechanical strength, can be repeatedly used and has long service life.
Drawings
FIG. 1: schematic preparation flow diagrams from original woven cloth to super-hydrophobic, super-hydrophilic and super-amphiphobic woven cloth obtained in examples 1, 2 and 3;
FIG. 2: a real figure of adding a silane coupling agent to the pretreatment solution, wherein (a) shows the TTOP-12 type silane coupling agent added in example 1, and (b) shows the KH550 type silane coupling agent added in examples 2 and 3;
FIG. 3: super-hydrophobic, super-hydrophilic and super-amphiphobic weaves wet and contact angle pictures of different solutions (water, tea, coffee, milk, oil), wherein, the graph (a) is the super-hydrophobic weaves of example 1, the graphs (a 1 and a 2) are the contact angle and rolling angle photos of water, the graph (b) is the super-hydrophilic weaves of example 2, the graphs (b 1 and b 2) are the contact angle of oil under water and the contact angle of water under oil, the graph (c) is the super-amphiphobic weaves of example 3, and the graphs (c 1 and c 2) are the contact angle of water and the contact angle of oil, respectively;
FIG. 4: scanning electron microscope pictures of the superhydrophobic fabric obtained in example 1;
FIG. 5: scanning electron microscope images of the surfaces of the woven fabrics obtained in examples 2 and 3, wherein the images (a) and (b) are the surfaces of the super-hydrophilic woven fabric obtained in example 2, and the images (c) and (d) are the surfaces of the super-amphiphobic fabric obtained in example 3;
FIG. 6: the test characterization of thermal stability, chemical stability, mechanical stability and ultraviolet stability of the superhydrophobic woven fabric obtained in example 1 and the superhydrophilic woven fabric obtained in example 2;
FIG. 7: an oil-water separator for the superhydrophobic woven fabric obtained in example 1 and the superhydrophilic woven fabric obtained in example 2;
FIG. 8: the oil-water separation efficiency, flux and circulation tests of the super-wet woven fabric obtained in the implementation are shown, wherein the graph (a) is the oil-water separation efficiency, flux and circulation tests of the super-hydrophobic woven fabric obtained in the example 1, and the graph (b) is the oil-water separation efficiency, flux and circulation tests of the super-hydrophilic woven fabric obtained in the example 2.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples. Various changes or modifications may be effected therein by one skilled in the art and such equivalents are intended to be within the scope of the invention as defined by the claims appended hereto.
Example 1:
1, pretreatment of woven fabric: 0.1mol/L zinc acetate is weighed and added into 50mL isopropanol to be heated and stirred, 0.1mol/L triethylamine is added to be mixed after dissolution, a milky white solution is formed, and then the solution is cooled to room temperature. Then weighing 20g of the solution, adding 1.5 wt% of hydrophobic silane coupling agent TTOP-12, stirring and mixing, adding the ultrasonically cleaned woven fabric, soaking for 5min, taking out, and airing at 120 ℃ for later use.
2, growth of nano zinc oxide: preparing 0.15mol/L zinc nitrate and 0.15mol/L hexamethylenetetramine aqueous solution, mixing 50mL of each aqueous solution, stirring for 30min to obtain a zinc oxide growth solution, vertically putting the pretreated woven fabric into the growth solution, reacting for 8h in an oil bath at 95 ℃, and standing for 12h at normal temperature to finish the growth of the nano zinc oxide.
3, low surface energy substance modification: and D, taking out the woven fabric in the step B, repeatedly washing with distilled water and then drying. And then soaking the woven fabric into 0.05mol/L stearic acid ethanol solution for 2 hours, washing with absolute ethyl alcohol, and drying in a vacuum drying oven at 60 ℃ to obtain the super-hydrophobic woven fabric.
Example 2:
1, pretreatment of woven fabric: 0.1mol/L zinc acetate is weighed and added into 50mL isopropanol to be heated and stirred, 0.1mol/L triethylamine is added to be mixed after dissolution, a milky white solution is formed, and then the solution is cooled to room temperature. Then weighing 20g of the solution, adding 2 wt% of hydrophilic silane coupling agent KH550, stirring and mixing, adding the ultrasonically cleaned woven fabric, soaking for 5min, taking out, and airing at 120 ℃ for later use.
2, growth of nano zinc oxide: preparing 0.05mol/L zinc nitrate and 0.05mol/L hexamethylenetetramine aqueous solution, mixing 50mL of each aqueous solution, stirring for 30min to obtain a zinc oxide growth solution, vertically putting the pretreated woven fabric into the growth solution, reacting for 8h in an oil bath at 95 ℃, and standing for 12h at normal temperature to finish the growth of the nano zinc oxide.
3, drying treatment: and (3) taking out the woven fabric in the step (2), repeatedly washing with distilled water and then drying. The super-hydrophilic fabric can be obtained without further treatment.
Example 3:
1, pretreatment of woven fabric: 0.1mol/L zinc acetate is weighed and added into 50mL isopropanol to be heated and stirred, 0.1mol/L triethylamine is added to be mixed after dissolution, a milky white solution is formed, and then the solution is cooled to room temperature. Then weighing 20g of the solution, adding 2 wt% of hydrophilic silane coupling agent KH550, stirring and mixing, adding the ultrasonically cleaned woven fabric, soaking for 5min, taking out, and airing at 120 ℃ for later use.
2, growth of nano zinc oxide: preparing 0.025mol/L zinc nitrate and 0.025mol/L hexamethylenetetramine aqueous solution, mixing 50mL of each aqueous solution, stirring for 30min to obtain a zinc oxide growth solution, vertically putting the pretreated woven fabric into the growth solution, reacting for 8h in an oil bath at 95 ℃, and standing for 12h at normal temperature to finish the growth of the nano zinc oxide.
3, low surface energy substance modification: and (3) taking out the woven fabric in the step (2), repeatedly washing with distilled water and then drying. And then soaking the woven fabric into 0.005mol/L perfluorooctanoic acid ethanol solution for 24 hours, washing with absolute ethyl alcohol, and drying in a vacuum drying oven at 60 ℃ to obtain the super-amphiphobic woven fabric.
The method comprises the steps of pretreatment of the fabric, growth of the zinc oxide nano-rod, modification of a low surface energy substance and the like. The research realizes super-hydrophobic, super-hydrophilic and super-amphiphobic performances by controlling the growth of zinc oxide on the woven fabric and selecting different modifiers, and has good stability under heating, acid-base, abrasion experiments and ultraviolet irradiation. In addition, the paper can be used for separating oil-water mixture, not only can realize the separation of light oil, heavy oil and water, but also can realize the separation of oil and water according to the requirement. The preparation method disclosed by the invention is simple in preparation process, controllable, easy to obtain, strong in stability, suitable for large-area preparation and application, suitable for application in daily life, and also suitable for industrial fields such as oil-water separation and the like.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.

Claims (1)

1. A method for producing a super-wet woven fabric having excellent stability and resistance for oil-water separation, comprising the steps of:
A. pretreatment of weaving: weighing zinc acetate, adding the zinc acetate into isopropanol, heating and stirring, dissolving, adding triethylamine, mixing, wherein the concentrations of the zinc acetate and the triethylamine are both 0.1mol/L, forming a milky white solution, and cooling to room temperature; then weighing the solution, adding a hydrophobic titanate coupling agent TTOP-12, stirring and mixing to form a mixed solution A, or adding a hydrophilic silane coupling agent KH550, stirring and mixing to form a mixed solution B, wherein the ratio of the added titanate coupling agent TTOP-12 and the silane coupling agent KH550 to the pretreatment solution is 1.5 w% and 2 w%, respectively, adding the ultrasonically cleaned woven fabric into the solution A or the solution B, soaking for 5min, taking out, and airing at 120 ℃ for later use;
B. and (3) growth of nano zinc oxide: preparing zinc nitrate and hexamethylenetetramine aqueous solution with equal concentration, wherein the concentration of the zinc nitrate and the hexamethylenetetramine aqueous solution is 0.15mol/L or 0.05mol/L or 0.025mol/L, mixing in equal volume, stirring for 30min to obtain a zinc oxide growth solution, vertically putting the pretreated woven fabric into the growth solution, reacting for 8h in an oil bath at 95 ℃, and standing for 12h at normal temperature to finish the growth of the nano zinc oxide;
C. low surface energy substance modification: taking out the woven fabric in the step B, repeatedly washing with distilled water and then drying;
if the hydrophilic silane coupling agent KH550 is added in the pretreatment, the super-hydrophilic woven fabric can be obtained without further treatment;
if the hydrophobic titanate coupling agent TTOP-12 is added in the pretreatment, then the woven fabric is immersed into a stearic acid ethanol solution with the concentration of 0.05mol/L for 2h to obtain the super-hydrophobic performance; or if the hydrophilic silane coupling agent KH550 is added in the pretreatment, soaking the woven fabric into a perfluorooctanoic acid ethanol solution with the concentration of 0.005mol/L for 24 hours to obtain the super-amphiphobic property; and then taking out the woven fabric, washing the woven fabric with absolute ethyl alcohol, and drying the woven fabric in a vacuum drying oven at 60 ℃ to obtain the super-hydrophobic woven fabric or the super-amphiphobic woven fabric.
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